Tert-phenol-furfuryl amine type benzoxazine monomer, cured resin, and preparation method of copolymerized resin thereof

A benzoxazine and furfurylamine type technology, applied in the field of organic polymer materials, can solve problems such as not being able to meet requirements well, achieve good thermal performance, reduce dielectric constant and dielectric loss, and improve thermal performance.

Pending Publication Date: 2020-03-10
淮北绿洲新材料有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the dielectric constant k of common benzoxazine resins is generally 3.5, and f is generally 0.02 (

Method used

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  • Tert-phenol-furfuryl amine type benzoxazine monomer, cured resin, and preparation method of copolymerized resin thereof
  • Tert-phenol-furfuryl amine type benzoxazine monomer, cured resin, and preparation method of copolymerized resin thereof
  • Tert-phenol-furfuryl amine type benzoxazine monomer, cured resin, and preparation method of copolymerized resin thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Under nitrogen protection, add 0.1mol p-tert-butylphenol, 0.1mol furfurylamine, and 0.2mol paraformaldehyde into a 250mL three-necked flask equipped with a condenser, magnetic stirring, and thermometer. The molar ratio is 2:1:1, then add 51mL xylene / butanone mixed solvent (the volume ratio is 3:1), mix well and heat to 80°C for 48h reaction, after the reaction, pour the reaction solution into 100mL methanol solution (concentration 80wt%) to obtain a suspension, let it stand for 24 hours, remove the supernatant to obtain a precipitate, dry the precipitate at 60°C for 8 hours in vacuum, and finally grind the dried product to obtain a powder that is tert-phenol-furfurylamine type benzoxazine monomer.

Embodiment 2

[0031] Under nitrogen protection, add 0.1mol furfurylamine and 0.2mol paraformaldehyde into a three-necked flask equipped with a condenser, magnetic stirring, and a thermometer, add 60mL of chloroform / methanol mixed solvent (the volume ratio is 1: 1), and mix After stirring for 1.5h, add 0.1mol p-tert-butylphenol, the molar ratio of aldehyde group, phenolic hydroxyl group and amino functional group is 2:1:1, heat to 120°C and continue the reaction for 4.5h, after the reaction is completed, pour the reaction solution into 100mL Obtain a suspension in a methanol solution (concentration 65wt%), let it stand for 24 hours, remove the supernatant to obtain a precipitate, dry the precipitate in vacuum at 60°C for 6 hours, and finally grind the dried product to obtain a powder that is tert-phenol-bran Amine type benzoxazine monomer.

Embodiment 3

[0033]Under the protection of nitrogen, add 0.1mol furfurylamine and 0.2mol paraformaldehyde into a three-necked flask equipped with a condenser, magnetic stirring, and a thermometer, and add 60mL of dioxane / ethyl acetate (the volume ratio is 1: 3 ), after mixing and stirring for 2 hours, add 0.1mol of p-tert-butylphenol, the molar ratio of aldehyde group, phenolic hydroxyl group and amino functional group is 2:1:1, heat at 110°C and continue to react for 12 hours, after the reaction, pour the reaction solution into 100mL Obtain a suspension in a methanol solution (concentration 70wt%), let it stand for 24 hours, remove the supernatant to obtain a precipitate, dry the precipitate in vacuum at 60°C for 12 hours, and finally grind the dried product to obtain a powder that is tert-phenol-bran Amine type benzoxazine monomer.

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Abstract

The invention relates to a tert-phenol-furfuryl amine type benzoxazine monomer, cured resin, and a preparation method of copolymerized resin thereof. The preparation method includes: in a one-time feeding or stepwise feeding manner, an aldehyde compound, furfuryl amine and p-tert-butylphenol are added into a reaction container, and an organic solvent is added for dissolution; then the mixture is heated to 80-120 DEG C and subjected to stirring reaction for 6-48 h, and the reaction product is subjected to after treatment to obtain the tert-phenol-furfuryl amine type benzoxazine monomer; the benzoxazine monomer then is dissolved in the solvent, and the mixture is heated to be heat-cured, thus preparing the tert-phenol-furfuryl amine type benzoxazine resin; or the benzoxazine monomer is subjected to dissolution and blending and subjected to thermo-curing with a benzoxazine prepolymer to obtain benzoxazine copolymerized resin. The method is low in cost and simple in process, wherein the tert-phenol-furfuryl amine type benzoxazine resin and the copolymerized resin thereof have great thermal property and excellent dielectric performance, i.e., low dielectric constant and dielectric lossunder ultrahigh frequency. The product can be applied to the fields such as high-frequency and high-speed circuit board substrate, micron wave and millimeter wave communication, vehicle-borne radars,and other composite materials.

Description

technical field [0001] The invention relates to the technical field of organic polymer materials, in particular to a preparation method of a tert-phenol-furfurylamine type benzoxazine monomer, a cured resin and a copolymerized resin thereof. Background technique [0002] In recent years, the widespread use of electronic terminal products such as mobile phones and car navigation, especially the emergence of the fifth-generation mobile communication system (5G), marks the beginning of the comprehensive information age. In order to meet the requirements of high-quality information transmission, the communication is constantly developing towards higher frequency and higher speed, which puts forward higher requirements for the electronic components and their carriers - copper clad laminates, which require a very low and stable dielectric The dielectric constant (k) and dielectric loss (f), and the dielectric properties of the matrix resin play a key role in the dielectric propert...

Claims

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Application Information

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IPC IPC(8): C07D413/06C08G14/06C08L61/34
CPCC07D413/06C08G14/06C08L61/34
Inventor 曾鸣陈江炳
Owner 淮北绿洲新材料有限责任公司
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